CN112893839A - Method for preparing Al1.2CoxCrFeNi high-entropy alloy through laser melting deposition - Google Patents
Method for preparing Al1.2CoxCrFeNi high-entropy alloy through laser melting deposition Download PDFInfo
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract
The invention discloses a method for preparing an Al 1.2CoxCrFeNi high-entropy alloy through laser melting deposition. The method is characterized by comprising the steps that five kinds of metal elementary substance powder of Al, Co, Cr, Fe and Ni are subjected to ball milling and mixed to be uniform according to the atomic ratio of 1.2: (2.2-2.8): 1:1:1, vacuum drying is conducted, and Al 1.2CoxCrFeNi high-entropy alloy powder is prepared; and then the mixed powder is subjected to multi-layer and multi-channel laser deposition additive preparation on a stainless steel substrate through lasers in a coaxial powder feeding manner, and the specific method for preparing the BCC/FCC dual-phase block high-entropy alloy is achieved. The mixed powder based on the atomic ratio is subjected to laser deposition, a BCC/FCC dual-phase high-entropy alloy structure can be generated, and a deposited high-entropy alloy block is good in density through detection and has high compression strength and tensile strength.
Description
Technical Field
The invention relates to the technical field of additive manufacturing, in particular to a method for preparing an Al1.2CoxCrFeNi high-entropy alloy by laser melting deposition.
Background
In recent years, high-entropy alloy has attracted much attention of many material researchers at home and abroad as a new multi-principal element material due to its excellent properties such as high hardness, high strength, high toughness, good wear resistance and high thermal stability. General material science theories believe that more added elements tend to form complex phases such as intermetallic compounds, which are detrimental to the performance of the alloy. However, it has been found through extensive experimentation that alloys of three or more principal elements can form stable solid solution phases rather than multiple complex phases. In 2004, Taiwan scholars, professor yesterday, etc. break away from the traditional alloy manufacturing concept and propose a multi-principal-element alloy design concept, namely 'high-entropy alloy'. Unlike typical alloys, the combination of elements produces no multi-phase or intermetallic compounds, but simple solid solution phases such as BCC, FCC, HCP, etc., which the leaf teaches is attributed to the high entropy of mixing created by the thermodynamic constraints of the multi-principal element system.
At present, the preparation method of the high-entropy alloy mainly adopts the traditional vacuum arc melting and fusion casting technology. Researches find that the high-entropy alloy prepared by arc melting has a simple solid solution structure and excellent mechanical properties. And the cooling speed of the electric arc melting is lower, the prepared alloy is easy to have the defects of macro segregation, shrinkage cavity and the like, and the period of preparing complex parts by the electric arc melting method and the casting method is longer, the utilization rate of raw materials is low, and the cost is high. Therefore, with the development of additive manufacturing technology, research on forming high-entropy alloys by using 3D printing technology has been favored by various researchers in recent years. The laser melting deposition material increase technology has the characteristic of rapid solidification after rapid melting, so that fine grain structures are easily obtained, the phenomena of segregation, uneven components and the like can be effectively inhibited, and the block alloy with more excellent performance can be prepared.
Disclosure of Invention
Aiming at the defects of the traditional preparation process, the invention provides a method for preparing the Al1.2CoxCrFeNi high-entropy alloy by laser melting deposition, and the prepared bulk high-entropy alloy has good density, higher hardness, compressive strength and tensile strength.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing Al1.2CoxCrFeNi high-entropy alloy by laser melting deposition is characterized in that: the method comprises the following steps:
1) polishing a stainless steel substrate by using an angle grinder to be smooth and clean before laser deposition so as to ensure that the surface does not contain substances which are not beneficial to deposition, such as oxides, oil stains and the like, cleaning the stainless steel substrate by using absolute ethyl alcohol, and then drying the stainless steel substrate in a drying box for later use;
2) preparing high-entropy alloy powder for laser additive manufacturing, wherein the high-entropy alloy powder is prepared from five metal elementary powder of Al, Co, Cr, Fe and Ni, the atomic ratio of the five metal elementary powder of the high-entropy alloy powder is 1.2 (2.2-2.8) to 1:1:1, the purity of the Al, Co, Cr, Fe and Ni is more than or equal to 99.5%, and the granularity is 150-300 meshes;
3) putting the prepared five metal simple substance powders into a planetary ball mill, ball-milling for 4 hours at a rotating speed of 100r/min to uniformly mix the powders, putting the ball-milled mixed powder into a vacuum drying oven, drying for two hours at 120 ℃, and taking out for later use;
4) argon with the purity of 99.99 percent is set as inert protective gas and is ensured to be sufficient, the diameter of a light spot is 1 mm-6 mm, the laser lap joint rate is 40-50 percent, the laser power is 1500W-2500W, the scanning speed is 5 mm/s-15 mm/s, the powder feeding speed is 0.6 rad/min-1.2 rad/min, and the protective gas flow is 15-25L/min;
5) after setting is finished, starting equipment to perform multilayer and multi-pass deposition on a 304 stainless steel substrate in a coaxial powder feeding mode under the protection of argon with the purity of 99.99 percent, and finally obtaining the Al1.2CoxCrFeNi high-entropy alloy block.
Further, the configuration of the step 3) also comprises the steps of putting five kinds of metal simple substance powder into a planetary ball mill stainless steel tank, and putting the powder into alumina balls with the diameters of 5mm and 8mm which are approximately the same as the volume of the powder for matching processing, wherein the mass ratio of the 5mm alumina balls to the 8mm alumina balls is 3:7
The beneficial technical effects are as follows:
compared with the traditional casting technology, five kinds of metal simple substance powder of Al, Co, Cr, Fe and Ni are prepared into Al1.2CoxCrFeNi high-entropy alloy powder according to the atomic ratio of 1.2 (2.2-2.8): 1:1:1 and through ball milling, uniform mixing and vacuum drying, and the mixed powder is subjected to multilayer multi-channel laser deposition material increase on a stainless steel substrate in a coaxial powder feeding mode to prepare the BCC/FCC dual-phase bulk high-entropy alloy.
Drawings
FIG. 1 is a sample diagram of the Al1.2Co2.2CrFeNi high-entropy alloy obtained in example 1.
FIG. 2 is a sample diagram of an Al1.2Co2.8CrFeNi high-entropy alloy obtained in example 2.
FIG. 3 is an SEM photograph of the Al1.2Co2.2CrFeNi high-entropy alloy obtained in example 1.
Fig. 4 is an SEM image of an al1.2co2.8crfeni high-entropy alloy obtained in example 2.
Fig. 5 is XRD spectra of al1.2co2.2crfeni and al1.2co2.8crfeni high-entropy alloys obtained in example 1 and example 2.
FIG. 6 is a graph comparing hardness distributions of the Al1.2Co2.2CrFeNi high-entropy alloy and the Al1.2Co2.8CrFeNi high-entropy alloy obtained in example 1 and example 2.
FIG. 7 is a graph showing a comparison of the compression properties of the Al1.2Co2.2CrFeNi high-entropy alloy and the Al1.2Co2.8CrFeNi high-entropy alloy obtained in examples 1 and 2.
FIG. 8 is a graph showing the tensile properties of the Al1.2Co2.2CrFeNi high-entropy alloy and the Al1.2Co2.8CrFeNi high-entropy alloy obtained in examples 1 and 2 in comparison.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflicting with each other.
Method for preparing Al1.2CoxCrFeNi high-entropy alloy by laser melting deposition as shown in FIGS. 1-8
A method for preparing Al1.2Co2.2CrFeNi high-entropy alloy by laser melting deposition comprises the following steps:
1. preparing Al, Co, Cr, Fe and Ni elementary substance powder with the purity of more than or equal to 99.5% according to the atomic ratio of 1.2:2.2:1:1:1, putting the prepared powder into a planetary ball mill stainless steel tank, putting alumina balls with the diameters of 5mm and 8mm which are approximately the same as the volume of the powder into the stainless steel tank, wherein the mass ratio of the 5mm alumina balls to the 8mm alumina balls is 3:7, and ball-milling for 4 hours at the rotating speed of 100r/min to uniformly mix the powder.
2. And putting the mixed powder subjected to ball milling into a vacuum drying oven, drying for two hours at the temperature of 120 ℃, and taking out for later use.
3. Polishing a 304 stainless steel substrate by using an angle grinder to ensure that the surface of the substrate is free of impurities which are not beneficial to deposition, such as oxides, oil stains, steel rust and the like, cleaning the substrate by using absolute ethyl alcohol, and then drying the substrate in a drying box for later use.
4. Pouring the alloy powder in the step 2 into a powder feeder and setting a laser deposition process as follows: the laser power is 2000W, the scanning speed is 10mm/s, the powder feeding speed is 1rad/min, and the diameter of a light spot is 4 mm. And performing multi-layer and multi-pass deposition on a 304 stainless steel substrate under the protection of argon with the purity of 99.99 percent to finally obtain the Al1.2Co2.2CrFeNi high-entropy alloy block.
Example 2
A method for preparing Al1.2Co2.8CrFeNi high-entropy alloy by laser melting deposition comprises the following steps:
1. preparing Al, Co, Cr, Fe and Ni elementary substance powder with the purity of more than or equal to 99.5% according to the atomic ratio of 1.2:2.2:1:1:1, putting the prepared powder into a planetary ball mill stainless steel tank, putting alumina balls with the diameters of 5mm and 8mm which are approximately the same as the volume of the powder into the stainless steel tank, wherein the mass ratio of the 5mm alumina balls to the 8mm alumina balls is 3:7, and ball-milling for 4 hours at the rotating speed of 100r/min to uniformly mix the powder.
2. And putting the mixed powder subjected to ball milling into a vacuum drying oven, drying for two hours at the temperature of 120 ℃, and taking out for later use.
3. Polishing a 304 stainless steel substrate by using an angle grinder to ensure that the surface of the substrate is free of impurities which are not beneficial to deposition, such as oxides, oil stains, steel rust and the like, cleaning the substrate by using absolute ethyl alcohol, and then drying the substrate in a drying box for later use.
4. Pouring the alloy powder in the step 2 into a powder feeder and setting a laser deposition process as follows: the laser power is 2000W, the scanning speed is 10mm/s, the powder feeding speed is 1rad/min, and the diameter of a light spot is 4 mm. And carrying out multi-layer and multi-pass deposition on a 304 stainless steel substrate under the protection of argon with the purity of 99.99 percent to finally obtain the Al1.2Co2.8CrFeNi high-entropy alloy block.
The high entropy alloy of the above example was subjected to hardness test, compression test and tensile test. The test results are shown in Table 1.
The hardness test method comprises the following steps: measuring the high-entropy alloy block by using an HVS-1000Z type microhardness instrument, and marking one point every 1mm from top to bottom, taking 25 points in total and calculating the average hardness value. The experimental parameters of the hardness tester are as follows: the experimental load was 1000g and the experimental loading time was 15 s.
The compression performance test method comprises the following steps: the cylindrical test sample for the compression experiment, the diameter is 5mm, the height is 10mm, the upper plane and the lower plane are parallel, the compression is carried out at room temperature by using a mechanical testing machine controlled by a computer, and the compression speed is set to be 1 mm/min.
The tensile property test method comprises the following steps: the dimensions of the compression test are shown in FIG. 8, the sample thickness of the compression test is 2mm, and the tensile test is carried out at room temperature using a computer-controlled mechanical testing machine, and the tensile speed is 1 mm/min.
TABLE 1 Properties of Al1.2CoxCrFeNi high entropy alloys of example 1 and example 2
Compared with the traditional casting technology, the invention realizes the preparation of the BCC/FCC dual-phase Al1.2CoxCrFeNi high-entropy alloy by laser melting deposition by using the characteristic of high energy density of laser. The obtained product has good density and good mechanical property, and lays a solid foundation for manufacturing high-entropy alloy complex parts.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (2)
1. A method for preparing Al1.2CoxCrFeNi high-entropy alloy by laser melting deposition is characterized in that: the method comprises the following steps:
1) polishing a stainless steel substrate by using an angle grinder to be smooth and clean before laser deposition so as to ensure that the surface does not contain substances which are not beneficial to deposition, such as oxides, oil stains and the like, cleaning the stainless steel substrate by using absolute ethyl alcohol, and then drying the stainless steel substrate in a drying box for later use;
2) preparing high-entropy alloy powder for laser additive manufacturing, wherein the five metal elementary powder of Al, Co, Cr, Fe and Ni are in an atomic ratio of 1.2: x:1:1:1, wherein the numerical value of x is set to be 2.2-2.8, the purity of Al, Co, Cr, Fe and Ni is more than or equal to 99.5%, and the granularity is 150-300 meshes;
3) putting the prepared five metal simple substance powders into a planetary ball mill, ball-milling for 4 hours at a rotating speed of 100r/min to uniformly mix the powders, putting the ball-milled mixed powder into a vacuum drying oven, drying for two hours at 120 ℃, and taking out for later use;
4) argon with the purity of 99.99 percent is set as inert protective gas and is ensured to be sufficient, the diameter of a light spot is 1-6 mm, the laser lap joint rate is 40-50 percent, the laser power is 1500-2500W, the scanning speed is 5-15 mm/s, the powder feeding speed is 0.6-1.2 rad/min, and the protective gas flow is 15-25L/min;
5) after setting is finished, starting equipment to perform multilayer and multi-pass deposition on a 304 stainless steel substrate in a coaxial powder feeding mode under the protection of argon with the purity of 99.99 percent, and finally obtaining the Al1.2CoxCrFeNi high-entropy alloy block.
2. The method for preparing the Al1.2CoxCrFeNi high-entropy alloy by laser melting deposition as claimed in claim 1, wherein: the configuration of the step 3) further comprises the steps of putting five kinds of metal simple substance powder into a planetary ball mill stainless steel tank, and putting the powder into alumina balls which are approximately same as the powder in volume and have the diameters of 5mm and 8mm respectively for matching processing, wherein the mass ratio of the 5mm alumina balls to the 8mm alumina balls is 3: 7.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113751722A (en) * | 2021-08-17 | 2021-12-07 | 温州大学 | Method for preparing FCC phase high-entropy alloy with high strength and high toughness |
| CN114875288A (en) * | 2022-04-08 | 2022-08-09 | 江苏大学 | High-entropy alloy reinforced high-speed steel wear-resistant material and preparation method thereof |
| CN115505811A (en) * | 2022-08-18 | 2022-12-23 | 华南理工大学 | Al-Cr-Co-Ni high-entropy alloy and preparation method and application thereof |
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